CN101481104A - Method for producing high purity battery level ferric pyrophosphate from pickle liquor - Google Patents
Method for producing high purity battery level ferric pyrophosphate from pickle liquor Download PDFInfo
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- CN101481104A CN101481104A CNA2009101053359A CN200910105335A CN101481104A CN 101481104 A CN101481104 A CN 101481104A CN A2009101053359 A CNA2009101053359 A CN A2009101053359A CN 200910105335 A CN200910105335 A CN 200910105335A CN 101481104 A CN101481104 A CN 101481104A
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- pickle liquor
- ferric phosphate
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- phosphate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a method for producing high-purity battery pole ferric phosphate by adopting pickle liquor, which comprises the following steps: adding iron sheet or scrap iron inside a reactive tank, pouring the pickle liquor; filtering the mixture to obtain purified ferrite solution; adding the purified ferrite solution inside a catalytic reaction kettle, and adding oxidant to perform exothermal reaction; dissolving and stirring phosphate to obtain primary ferric phosphate sizing agent; separating the primary ferric phosphate sizing agent to obtain primary ferric phosphate filter mass; dissolving and stirring the filter mass to obtain primary ferric phosphate mixed solution; heating, insulating and stirring the mixture inside an insulation reaction kettle until the mixture becomes pink; inputting all the mixed solution to the insulation reaction kettle, insulating and stirring the mixed solution for a certain period of time; and separating the ferric phosphate inside the ground paste to obtain the finished product of ferric phosphate. The invention utilizes the industrial pickle liquor as the raw material of the production method, realizes the further development of the recycling economy and the green economy due to the circulation use of the industrial waste, and greatly lowers the production cost.
Description
Technical field
The present invention relates to a kind of production method of Orthophosphoric acid Ferrum, refer more particularly to a kind of method of utilizing waste pickle liquor to produce high purity battery level ferric pyrophosphate.
Background technology
Orthophosphoric acid Ferrum FePO
42H
2O, major ingredient are FePO
4The production technique of existing Orthophosphoric acid Ferrum generally is with phosphoric acid salt directly and the ferrous salt solution generation Orthophosphoric acid Ferrum that reacts, its products obtained therefrom particle diameter is thick, and size distribution is extremely inhomogeneous, total iron content is low, and Fe＜28% generally has only 22-26%, can produce spent pickle liquors in a large number during existing in addition industrial production degreasing and rust removal, the environment that the mankind are depended on for existence has caused serious pollution.
For these reasons, the inventor has developed the present invention's a kind of " utilizing waste pickle liquor to produce the method for high purity battery level ferric pyrophosphate ".
Summary of the invention
The present invention is directed to above-mentioned the deficiencies in the prior art technical problem to be solved is: provide the production method of a kind of ultra tiny, high purity, battery level ferric pyrophosphate, the FePO that it obtains
42H
2O finished product purity height, particle is tiny and even, and crystalline structure is reasonable.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of method of utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate, this method may further comprise the steps:
(a), in reactive tank, add iron plate or iron filings, pour spent pickle liquor into, be heated 95 ± 5 ℃, obtain ferrous salt solution, control its reacted spent acid amount≤1%, PH 〉=3.5;
(b), with ferrous salt solution by a set filter, fully filter its metallic impurity and nonmetallic impurity, remove metal simple-substance, make it obtain purified ferrous salt solution;
(c), in catalytic reaction kettle, add purified ferrous salt solution, adjust PH after, add oxygenant, make it that thermopositive reaction take place, controlling its temperature is 50 ± 5 ℃, PH≤4;
(d), dissolved phosphorus hydrochlorate and it is joined in the catalytic reaction kettle and powerful the stirring, adjust pH value, controlling its temperature is 50 ± 5 ℃, PH≤4 obtain primary ferric phosphate sizing agent;
(e), separate Orthophosphoric acid Ferrum and mother liquor in the primary ferric phosphate sizing agent, obtain primary ferric phosphate filter mass;
(f), in the conversion reaction still, add phosphoric acid (H
3PO
4) aqueous solution, primary ferric phosphate filter mass is put into dissolving and stirring in the conversion reaction still, obtain primary ferric phosphate mixed solution;
(g), a part of getting above-mentioned primary ferric phosphate mixed solution is transported to heat temperature raising to 75 in the insulation reaction still ± 5 ℃, insulation is also stirred the regular hour, becomes pink until color;
(h) all the other mixing solutionss all are input in the above insulation reaction still, insulation is also stirred the regular hour, becomes pink until the color of whole materials, can obtain the Orthophosphoric acid Ferrum slip;
(i) Orthophosphoric acid Ferrum in the separation slip obtains the Orthophosphoric acid Ferrum finished product through rinsing, drying and pulverizing process then.
Described step (a) and (b) in ferrous salt comprise ferrous sulfate, Iron nitrate and iron protochloride.
Oxygenant in the described step (c) is hydrogen peroxide, clorox, potassium hypochlorite, sodium chlorate, the Potcrate of technical grade or analytical pure level.
Phosphoric acid salt in the described step (d) is industrial grade phosphate or food-grade phosphate, and phosphoric acid salt comprises crystal water or anhydrous tertiary sodium phosphate (Na
3PO
4), DAP (NH
4)
2HPO
4Or ammonium di-hydrogen phosphate NH
4H
2PO
4
Phosphoric acid in the described step (f) comprises PHOSPHORIC ACID TECH.GRADE and analytical pure phosphoric acid.
Described described step (a) and (b) in the ferrous salt solution making method be:
1) spent pickle liquor that will contain ferrous ion adds scrap iron sheet or waste iron filing and is heated to 95 ± 5 ℃ of reaction consumes and falls unnecessary acid, control spent acid amount≤1%, and PH 〉=3.5 obtain ferrous iron solution;
2) ferrous iron solution is passed through one group of y-type filter or accurate filter and magnetic filter, fully filter its metallic impurity and nonmetallic impurity, remove iron filings, obtain purified ferrous salt solution, get its clear liquor as the ferrous salt solution of producing Ferrox.
Described step (g) and (h) in two steps that were converted into transform, it is that a part of getting primary ferric phosphate mixed solution is transported to heat temperature raising to 75 in the insulation reaction still ± 5 ℃ that the first step transforms, insulation is also stirred the regular hour, becomes pink until color; It is that all the other mixing solutionss all are input in the above insulation reaction still that second step transformed, and insulation is also stirred the regular hour, becomes pink until the color of whole materials, obtains the Orthophosphoric acid Ferrum slip.
Described step (a) and (b) in the concentration of ferrous salt solution be 50-800mg/l.
The production method of the Orthophosphoric acid Ferrum that the present invention relates to comprises catalysis [crying " oxidation " again], transforms [also claiming " wearing out "], separation and aftertreatment four big steps, wherein oxidizing reaction is for adding ferrous salt solution in catalytic reaction kettle, add oxygenant, make it that thermopositive reaction take place, the dissolved phosphate solution is joined in the catalytic reaction kettle, drip soda ash solution or ammonia and adjust the pH value of reaction soln, and separate mother liquor after powerful the stirring, it writes a Chinese character in simplified form reaction formula is Fe
2++ H
2O
2=Fe
3++ H
2O.Fe
3++ PO
4 3-=FePO
4
Conversion also claims aging, and the present invention adopts two step conversion methods, and the primary ferric phosphate filter mass that is about to gained in the oxidising process joins phosphoric acid (H
3PO
4) make mixing solutions in the solution, get one portion and be input to stirring and insulation certain hour in the insulation reaction still, treat again all the other mixing solutionss all to be input to stirring and insulation in the insulation reaction still after its pulverize redness, till the whole pulverize redness of material, mother liquor in the separating slurry afterwards, the rinsing drying, get final product after the pulverizing Orthophosphoric acid Ferrum (FePO
42H
2O) finished product.The Orthophosphoric acid Ferrum that aforesaid method obtains, particle diameter is tiny evenly, and the purity height is a desirable feedstock of making the lithium Fe battery positive electrode material.
With respect to prior art, the method beneficial effect that the present invention utilizes spent pickle liquor to produce high purity battery level ferric pyrophosphate is:
The method that adopts catalysis and two steps to transform makes its sufficient reacting, and reactivity improves greatly, the Orthophosphoric acid Ferrum finished product purity height that obtains, and particle diameter is tiny evenly.The Orthophosphoric acid Ferrum total iron content that obtains by production method of the present invention is more than the 28%--29%, particle diameter D
50≤ 10um, P 〉=16% utilizes the raw material of industrial acid-washed waste liquid as production method involved in the present invention in addition, utilizes the recycle of industrial waste, has realized the synchronized development of recycling economy and green economy, has both improved environment, greatly reduces production cost again.
Embodiment
Below in conjunction with embodiment the method for utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate that the technical program provides is described further.
The present invention implements like this:
The production method of the Orthophosphoric acid Ferrum that the present invention relates to comprises catalysis [crying " oxidation " again], transforms [also claiming " wearing out "], separation and aftertreatment four big steps, wherein oxidizing reaction is for adding ferrous salt solution in catalytic reaction kettle, add oxygenant, make it that thermopositive reaction take place, the dissolved phosphate solution is joined in the catalytic reaction kettle, drip soda ash solution or ammonia and adjust the pH value of reaction soln, and separate mother liquor after powerful the stirring, it writes a Chinese character in simplified form reaction formula is Fe
2++ H
2O
2=Fe
3++ H
2O.Fe
3++ PO
4 3-FePO
4
Conversion also claims aging, and the present invention adopts two step conversion methods, and the primary ferric phosphate filter mass that is about to gained in the oxidising process joins phosphoric acid (H
3PO
4) make mixing solutions in the solution, get one portion and be input to stirring and insulation certain hour in the insulation reaction still, treat again all the other mixing solutionss all to be input to stirring and insulation in the insulation reaction still after its pulverize redness, till the whole pulverize redness of material, mother liquor in the separating slurry afterwards, the rinsing drying, get final product after the pulverizing Orthophosphoric acid Ferrum (FePO
42H
2O) finished product.
The Orthophosphoric acid Ferrum that aforesaid method obtains, particle diameter is tiny evenly, and the purity height is a desirable feedstock of making the lithium Fe battery positive electrode material.
Further, in the Orthophosphoric acid Ferrum production process of the present invention, step (a) and (b) described in ferrous salt solution, comprise ferrous sulfate, Iron nitrate, iron protochloride, its making method is: 1. add iron plate or iron filings in reactive tank, pour waste pickle liquor into, be heated 95 ± 5 ℃, control its reacted spent acid amount≤1%, PH 〉=3.5; 2. ferrous salt solution is passed through one group of y-type filter or accurate filter and magnetic filter, fully filter its metallic impurity and nonmetallic impurity, remove metal simple-substance, can obtain the purified ferrous salt solution of producing Orthophosphoric acid Ferrum that can be used as.
Oxygenant in the step (c) comprises hydrogen peroxide, clorox, potassium hypochlorite or sodium chlorate, Potcrate of technical grade and analytical pure level or the like.
Phosphoric acid salt described in the step (d) comprises technical grade and food grade, contains crystal water or anhydrous tertiary sodium phosphate (Na
3PO
4), DAP (NH
4)
2HPO
4, ammonium di-hydrogen phosphate NH
4H
2PO
4With other phosphoric acid salt.
Embodiment 1, the production method of Orthophosphoric acid Ferrum:
A kind of method of utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate, this method may further comprise the steps:
(a), in reactive tank, add iron plate or iron filings, pour spent pickle liquor into, be heated 90 ℃, obtain ferrous salt solution, control its reacted spent acid amount≤1%, PH=3.5;
(b), with ferrous salt solution by a set filter, fully filter its metallic impurity and nonmetallic impurity, remove metal simple-substance, make it obtain purified ferrous salt solution;
(c), in catalytic reaction kettle, add purified ferrous salt solution, adjust PH after, add oxygenant, make it that thermopositive reaction take place, controlling its temperature is 45 ℃, PH=3.5;
(d), dissolved phosphorus hydrochlorate and it is joined in the catalytic reaction kettle and powerful the stirring, adjust pH value, controlling its temperature is 46 ℃, PH=3.5 obtains primary ferric phosphate sizing agent;
(e), separate Orthophosphoric acid Ferrum and mother liquor in the primary ferric phosphate sizing agent, obtain primary ferric phosphate filter mass;
(f), in the conversion reaction still, add phosphoric acid (H
3PO
4) aqueous solution, primary ferric phosphate filter mass is put into dissolving and stirring in the conversion reaction still, obtain primary ferric phosphate mixed solution;
(g), a part of getting above-mentioned primary ferric phosphate mixed solution is transported in the insulation reaction still heat temperature raising to 71 ℃, insulation is also stirred the regular hour, becomes pink until color;
(h) all the other mixing solutionss all are input in the above insulation reaction still, insulation is also stirred the regular hour, becomes pink until the color of whole materials, can obtain the Orthophosphoric acid Ferrum slip;
(i) Orthophosphoric acid Ferrum in the separation slip obtains the Orthophosphoric acid Ferrum finished product through rinsing, drying and pulverizing process then.
Embodiment 2, the production method of Orthophosphoric acid Ferrum:
A kind of method of utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate, this method may further comprise the steps:
(a), in reactive tank, add iron plate or iron filings, pour spent pickle liquor into, be heated 100 ℃, obtain ferrous salt solution, control its reacted spent acid amount≤1%, PH=4;
(b), with ferrous salt solution by a set filter, fully filter its metallic impurity and nonmetallic impurity, remove metal simple-substance, make it obtain purified ferrous salt solution;
(c), in catalytic reaction kettle, add purified ferrous salt solution, adjust PH after, add oxygenant, make it that thermopositive reaction take place, controlling its temperature is 55 ℃, PH=4;
(d), dissolved phosphorus hydrochlorate and it is joined in the catalytic reaction kettle and powerful the stirring, adjust pH value, controlling its temperature is 55 ℃, PH=4 obtains primary ferric phosphate sizing agent;
(e), separate Orthophosphoric acid Ferrum and mother liquor in the primary ferric phosphate sizing agent, obtain primary ferric phosphate filter mass;
(f), in the conversion reaction still, add phosphoric acid (H
3PO
4) aqueous solution, primary ferric phosphate filter mass is put into dissolving and stirring in the conversion reaction still, obtain primary ferric phosphate mixed solution;
(g), a part of getting above-mentioned primary ferric phosphate mixed solution is transported in the insulation reaction still heat temperature raising to 80 ℃, insulation is also stirred the regular hour, becomes pink until color;
(h) all the other mixing solutionss all are input in the above insulation reaction still, insulation is also stirred the regular hour, becomes pink until the color of whole materials, can obtain the Orthophosphoric acid Ferrum slip;
(i) Orthophosphoric acid Ferrum in the separation slip obtains the Orthophosphoric acid Ferrum finished product through rinsing, drying and pulverizing process then.
Production method involved in the present invention after testing is more than the 28%--29% with the product total iron content that obtains, particle diameter D
50≤ 10um, P 〉=16%, further, utilize the raw material of industrial acid-washed waste liquid, utilize the recycle of industrial waste, realized the synchronized development of recycling economy and green economy as production method involved in the present invention, improve environment, greatly reduced production cost.
In the reactor that the 2000L band stirs, adding iron concentration is the ferrous salt solution shown in the following table, in the process that stirs, add hydrogen peroxide, dissolved phosphoric acid salt is joined in the catalytic reaction kettle, and add the primary products that ammonia adjusting pH value obtains Orthophosphoric acid Ferrum, its filter cake is joined phosphoric acid (H
3PO
4) short its of solution carry out two-step approach and transform, the control pH value, stir and insulation certain hour pulverize redness after separate, rinsing, drying, pulverize get final product Orthophosphoric acid Ferrum (FePO
42H
2O) finished product.Below be every reaction numerical value from embodiment 1 to embodiment 6.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Ferrous salt iron concentration Mg/l | 180 | 200 | 220 | 240 | 260 | 280 |
| PH value after the oxidizing reaction | 4.3 | 4.5 | 4.4 | 4.3 | 4.2 | 4.5 |
| Oxidizing reaction temperature | 55 | 52 | 48 | 49 | 53 | 54 |
| PH value and temperature after transforming for the first time | 2/75 | 2/71 | 1.8/74 | 2/78 | 2.2/79 | 2/76 |
| PH and temperature after transforming for the second time | 1.5/78 | 1.6/77 | 1.7/76 | 1.8/75 | 1.6/77 | 1.5/78 |
| Soaking time (h) | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 |
The above, only be that the present invention utilizes spent pickle liquor to produce the method preferred embodiment of high purity battery level ferric pyrophosphate, be not that technical scope of the present invention is imposed any restrictions, every foundation technical spirit of the present invention all still belongs in the scope of technical solution of the present invention above any trickle modification, equivalent variations and modification that embodiment did.
Claims (8)
1. method of utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate, this method may further comprise the steps:
(a), in reactive tank, add iron plate or iron filings, pour spent pickle liquor into, be heated 95 ± 5 ℃, obtain ferrous salt solution, control its reacted spent acid amount≤1%, PH 〉=3.5;
(b), with ferrous salt solution by a set filter, fully filter its metallic impurity and nonmetallic impurity, remove metal simple-substance, make it obtain purified ferrous salt solution;
(c), in catalytic reaction kettle, add purified ferrous salt solution, adjust PH after, add oxygenant, make it that thermopositive reaction take place, controlling its temperature is 50 ± 5 ℃, PH≤4;
(d), dissolved phosphorus hydrochlorate and it is joined in the catalytic reaction kettle and powerful the stirring, adjust pH value, controlling its temperature is 50 ± 5 ℃, PH≤4 obtain primary ferric phosphate sizing agent;
(e), separate Orthophosphoric acid Ferrum and mother liquor in the primary ferric phosphate sizing agent, obtain primary ferric phosphate filter mass;
(f), in the conversion reaction still, add phosphoric acid (H
3PO
4) aqueous solution, primary ferric phosphate filter mass is put into dissolving and stirring in the conversion reaction still, obtain primary ferric phosphate mixed solution;
(g), a part of getting above-mentioned primary ferric phosphate mixed solution is transported to heat temperature raising to 75 in the insulation reaction still ± 5 ℃, insulation is also stirred the regular hour, becomes pink until color;
(h) all the other mixing solutionss all are input in the above insulation reaction still, insulation is also stirred the regular hour, becomes pink until the color of whole materials, can obtain the Orthophosphoric acid Ferrum slip;
(i) Orthophosphoric acid Ferrum in the separation slip obtains the Orthophosphoric acid Ferrum finished product through rinsing, drying and pulverizing process then.
2. the method for utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate according to claim 1, it is characterized in that described step (a) and (b) in ferrous salt comprise ferrous sulfate, Iron nitrate and iron protochloride.
3. the method for utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate according to claim 1 is characterized in that the oxygenant in the described step (c) is hydrogen peroxide, clorox, potassium hypochlorite, sodium chlorate, the Potcrate of technical grade or analytical pure level.
4. the method for utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate according to claim 1 is characterized in that the phosphoric acid salt in the described step (d) is industrial grade phosphate or food-grade phosphate, and phosphoric acid salt comprises crystal water or anhydrous tertiary sodium phosphate (Na
3PO
4), DAP (NH
4)
2HPO
4Or ammonium di-hydrogen phosphate NH
4H
2PO
4
5. the method for utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate according to claim 1 is characterized in that the phosphoric acid in the described step (f) comprises PHOSPHORIC ACID TECH.GRADE and analytical pure phosphoric acid.
6. the method for utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate according to claim 1, it is characterized in that described described step (a) and (b) in the ferrous salt solution making method be:
1) spent pickle liquor that will contain ferrous ion adds scrap iron sheet or waste iron filing and is heated to 95 ± 5 ℃ of reaction consumes and falls unnecessary acid, control spent acid amount≤1%, and PH 〉=3.5 obtain ferrous iron solution;
2) ferrous iron solution is passed through one group of y-type filter or accurate filter and magnetic filter, fully filter its metallic impurity and nonmetallic impurity, remove iron filings, obtain purified ferrous salt solution, get its clear liquor as the ferrous salt solution of producing Ferrox.
7. the method for utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate according to claim 1, it is characterized in that described step (g) and (h) in two steps that were converted into transform, it is that a part of getting primary ferric phosphate mixed solution is transported to heat temperature raising to 75 in the insulation reaction still ± 5 ℃ that the first step transforms, insulation is also stirred the regular hour, becomes pink until color; It is that all the other mixing solutionss all are input in the above insulation reaction still that second step transformed, and insulation is also stirred the regular hour, becomes pink until the color of whole materials, obtains the Orthophosphoric acid Ferrum slip.
8, the method for utilizing spent pickle liquor to produce high purity battery level ferric pyrophosphate according to claim 1, it is characterized in that described step (a) and (b) in the concentration of ferrous salt solution be 50-800mg/l.
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|---|---|---|---|
| CNA2009101053359A CN101481104A (en) | 2009-02-11 | 2009-02-11 | Method for producing high purity battery level ferric pyrophosphate from pickle liquor |
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| CN102695760A (en) * | 2009-09-18 | 2012-09-26 | A123系统公司 | Ferric phosphate and methods of preparation thereof |
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| CN104134787A (en) * | 2014-07-28 | 2014-11-05 | 湖南工程学院 | Synthetic method of multi-element doped lithium iron phosphate/carbon composite anode material |
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| CN104555974A (en) * | 2015-01-19 | 2015-04-29 | 浙江大学 | Method for preparing lithium iron phosphate and lithium iron pyrophosphate by taking mineral leaching tail liquor as iron source |
| CN105129757A (en) * | 2015-08-27 | 2015-12-09 | 东莞道汇环保科技有限公司 | Method for preparing battery grade iron phosphate through chemical nickel-plating waste liquid |
| CN105692576B (en) * | 2016-03-10 | 2017-05-03 | 三峡大学 | Method for preparing battery-grade FePO4 from industrial iron-containing waste |
| CN105692576A (en) * | 2016-03-10 | 2016-06-22 | 三峡大学 | Method for preparing battery-grade FePO4 from industrial iron-containing waste |
| CN105967161A (en) * | 2016-06-23 | 2016-09-28 | 成都翔羽科技有限公司 | Method for continuously preparing low-cost battery grade ferric phosphate by utilizing iron filings |
| CN105967161B (en) * | 2016-06-23 | 2018-01-09 | 成都翔羽科技有限公司 | A kind of method that low-cost cell-grade ferric orthophosphate is continuously prepared using iron filings |
| CN107611433A (en) * | 2017-09-19 | 2018-01-19 | 江苏荣信环保科技有限公司 | A kind of method for preparing battery-grade iron phosphate using heavy metal sewage sludge and heavy metal spent acid |
| CN107611433B (en) * | 2017-09-19 | 2020-09-04 | 江苏荣信环保科技有限公司 | Method for preparing battery-grade iron phosphate by using heavy metal sludge |
| CN110002420A (en) * | 2019-05-07 | 2019-07-12 | 江西赣锋锂业股份有限公司 | A method of anhydrous iron phosphate is prepared using steel plant's pickle liquor |
| CN112142025A (en) * | 2019-06-26 | 2020-12-29 | 湖北虹润高科新材料有限公司 | Novel method capable of flexibly improving iron phosphate to phosphorus ratio |
| CN113023700A (en) * | 2019-12-24 | 2021-06-25 | 河南省净寰新能源科技有限公司 | Preparation method of high-purity nanoscale iron phosphate |
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